CN104036972A - Microwave preparation method for 3D zinc-aluminum double-metal hydroxides, and application in super capacitor - Google Patents
Microwave preparation method for 3D zinc-aluminum double-metal hydroxides, and application in super capacitor Download PDFInfo
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- CN104036972A CN104036972A CN201310068899.6A CN201310068899A CN104036972A CN 104036972 A CN104036972 A CN 104036972A CN 201310068899 A CN201310068899 A CN 201310068899A CN 104036972 A CN104036972 A CN 104036972A
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
Abstract
The invention belongs to the chemical field, and provides a microwave preparation method for 3D zinc-aluminum double-metal hydroxides, and an application in a super capacitor. Compared to the prior art, during the microwave preparation of the 3D double-metal hydroxides, the reaction is rapid, the energy consumption is small, and the yield can reach 98%. The 3D double-metal hydroxides obtained by use of the method have the advantages of larger specific surface, smaller mass transfer resistance and better structural stability. Besides, the synthesized 3D zinc-aluminum double-metal hydroxides are applied to the electrode material of the super capacitor, and the cost and the performance are better than the cost and performance of conventional precious metal oxides.
Description
Technical field
The invention belongs to chemical field, particularly a kind of microwave preparation of 3D zinc-aluminium double-metal hydroxide and the application in ultracapacitor.
Background technology
Ultracapacitor is a kind of novel energy storage/conversion equipment, has high energy density and power density, is expected to be applied to the every field of national defence, machinery, electronics and current consumption.According to energy storage mechanism need not, ultracapacitor can be divided into double electric layer capacitor and pseudo capacitance device.The former utilizes electronics and ion or dipole to store electric charge at the produced electric double layer of aligning of electrode/solution surface, and latter is in the accurate two-dimensional space of electrode surface or body phase, the pseudo capacitance that chemisorbed, desorption or redox reaction cause to occur by electroactive substance.In the situation that identical volume or weight, pseudo capacitance specific capacitance often 10～100 times of electric double layer capacitance specific capacitance above (Hao Jiang, Jan Ma and Chunzhong Li, Chem.Commun., 2012,48,4465-4467).Therefore, the performance of electrode material directly determines the energy storage quality of capacitor.
Tradition is prepared zinc-aluminium double-metal hydroxide and be take hydro thermal method as main, and this method property consuming time in building-up process is long, complex steps, and productive rate is also undesirable.Microwave is a kind of electromagnetic wave, and it can produce Electric and magnetic fields in space, and causes that in material, polar molecule changes polarised direction, thereby makes molecular motion aggravation obtain heat energy.Compare with traditional hydro thermal method, microwave method is easy to reappear, controllability is strong and method of operation is simple, as a kind of Performances of Novel Nano-Porous grain synthetic method, and not only environmental protection, nontoxicity, and there is distinctive high reaction efficiency.
At present, the material that is applied to ultracapacitor mainly contains carbon-based material (active carbon, carbon nano-tube, charcoal-aero gel, Graphene), transition metal oxide or hydroxide and conducting polymer (polyaniline).All there are pluses and minuses separately in different materials, as carbon-based material has great specific area, minimum electric double layer spacing and high cycle life, but pseudo capacitance is too low.Conducting polymer is cheap, but thermal stability, chemical stability and recyclability are poor, has limited to a certain extent its application.Double-metal hydroxide is a class formation high-sequential and the material that has multiple excellent function, and ionic bond, covalent bond, hydrogen bond, electrostatic force and Van der Waals force thereof interact therebetween.Due to the special layer structure of hydrotalcite, interlayer anion diversity and adjustability, for developing rapidly, this type of material provides broad space, can be used as novel high-performance super capacitor (Zhang Fang, former Changzhou, Zhang Jiaogang, Zhang Luojiang, Xu Ke, Acta PhySico-Chimica Sinica, 2010,26 (12): 3175-3180).Zinc-aluminium double-metal hydroxide is extensive, cheap because of raw material sources, is subject to the extensive attention of Chinese scholars.Yet, zinc-aluminium duplex metal hydroxide nanometer particle prepared by prior art is easily gathered into larger particles, the specific surface of material is reduced, and electrolyte can not fully contact with electroactive composition, thereby cause the super capacitor performance of this material significantly to reduce, can not meet the needs of high property super capacitor, and synthesis cycle is long, has affected actual applying.Therefore, set up a kind of microwave preparation of 3D zinc-aluminium double-metal hydroxide imperative.
Summary of the invention
The technical problem to be solved in the present invention be exactly long for existing zinc-aluminium double-metal hydroxide synthesis cycle, productive rate is low, nano particle is reunited serious and in electrochemical reaction the slow deficiency of mass transfer velocity, a kind of microwave preparation of 3D zinc-aluminium double-metal hydroxide is provided.Method has improved significantly the specific surface of zinc aluminum bimetal hydroxide composite material, the stability of structure and controllability, also environmental protection, and productive rate is high, and synthesis cycle is short.Can not cause environmental pollution.
The inventor finds through research widely and test repeatedly, by microwave method, prepare 3D zinc-aluminium double-metal hydroxide, it has not only realized the quick preparation of zinc-aluminium double-metal hydroxide, and between the nano particle of zinc-aluminium double-metal hydroxide, interlaced braiding forms specific 3d space structure, this has stoped the reunion of nano particle in material effectively, and has improved the mass transfer velocity of electrolyte and electroactive composition.The more important thing is, this method synthetic yield is high, and less energy consumption is conducive to suitability for industrialized production application.
The present invention solves the problems of the technologies described above adopted technical scheme: a kind of microwave preparation of 3D zinc-aluminium double-metal hydroxide and the application in ultracapacitor, comprise
1) by zinc and aluminium salt precursor body and organic solvent mixing, ultrasonic dispersion, is transferred in microwave reaction device.Set reaction temperature, microwave power and reaction time, open microwave, stir until system starts to reflux.
2) alkali source compound and organic solvent are mixed, are added to 1) in the backflow system of reacting, after stirring reaction, centrifugation, collecting precipitation, absolute ethanol washing, vacuumize.
3) by 2) the 3D zinc-aluminium double-metal hydroxide that makes, acetylene black and polytetrafluoroethylene mix, and stirs, and be then applied to bubble Zhu zinc surface, and be assembled into ultracapacitor.
Step 1) described zinc and aluminium salt precursor body are to be selected from any in the sulfate that contains positive divalent zinc ion or positive trivalent aluminium ion or nitrate.
Step 1) zinc described in and aluminium salt preferably amount of substance ratio are 3: 1～1: 3.
Step 1) described microwave reaction device refers to and can launch stability microwave and with the microwave device of agitating function.
Step 1) 50～80 ℃ respectively of the described better reaction temperature of microwave, microwave power and times, 200W-500W and 0.5～1.0h.
Step 2) described organic solvent is any of absolute ethyl alcohol, propyl alcohol, isopropyl alcohol or the tert-butyl alcohol, or their mixture.
Step 2) described zinc and aluminium salt precursor body and organic solvent quality 1: 50～1: 150 preferably.
Step 2) described alkali source compound is to be selected from any in the organic or inorganic compound that can decompose rapidly and discharge ammonia under hydrothermal condition, or their mixture.
Step 2) described alkali source compound and the mass ratio of organic solvent are 1: 10～1: 20.
Step 3) the 3D zinc-aluminium double-metal hydroxide described in and acetylene black, polytetrafluoroethylene preferably mass ratio are 1: 0.3: 0.15～1: 0.1: 0.05.
Step 3) barrier film that described assembling super capacitor is used is to be selected from any in the barrier film series that polypropylene material makes.The electrolyte potassium hydroxide solution that described assembling super capacitor is used.Described potassium hydroxide electrolyte solution preferred concentration is 3～6mol/L.
The microwave preparation of a kind of 3D zinc-aluminium double-metal hydroxide of the present invention and one preferred embodiment of the application in ultracapacitor comprise the following steps:
1) take 0.582g Zn (NO
3)
26H
2o and 0.873g Al (NO
3)
39H
2o, in 150mL absolute ethyl alcohol, is placed in microwave reaction device, opens microwave, sets 50 ℃ of reaction temperature lower limits, and 80 ℃ of the upper limits regulate microwave power 200W-500W, and the reaction time, stirring and dissolving reaction system was until system starts backflow at 0.5-1.0h.
2) slowly dropwise add the pre-configured ethanol-ammoniacal liquor of 10mL (V: V=10: 1) mixed solution, adjusting microwave power 300W left and right, controls 0.5h dropping and finish, successive reaction 1h.
3) experiment finishes, and closes microwave, and room temperature is cooling, vacuum filtration, and ethanol washing 5 times, 70 ℃ of dry 12h of vacuum, obtain 3D zinc-aluminium double-metal hydroxide.
4) electrode preparation.Weigh after 30mg3D zinc-aluminium double-metal hydroxide and 2.53～5.6mg acetylene black are mixed and grind, add a little binding agent PTFE (15%), with the ultrasonic dispersion of a small amount of absolute ethyl alcohol 30min, after dispersion, be coated in foam zinc surface, at 60～105 ℃, after vacuumize 6～12h, obtained required electrode slice.
In this preferred embodiment, zinc salt presoma, aluminium salt precursor body and alkali source compound microwave method are prepared 3D zinc-aluminium double-metal hydroxide respectively.Research shows, between the nano particle of zinc-aluminium double-metal hydroxide, interlaced braiding forms specific 3d space structure, is similar to honeycomb shape.Resulting 3D zinc-aluminium double-metal hydroxide is as the electrode material of ultracapacitor, and specific capacitance is at 500.2Fg
-1above, after circulation charge-discharge 1000 times, its capacity can also keep more than 96%.
The raw material that the present invention is used or reagent except special instruction, equal commercially available obtaining.
Each preferred version of the present invention can be used in combination mutually.
Compared with prior art, the present invention has following significant advantage:
(1) the present invention is by having prepared the 3D zinc-aluminium double-metal hydroxide with unique steric configuration without template microwave technology.Elementary cell in this structure is ultra-thin zinc-aluminium duplex metal hydroxide nanometer sheet, and they itself have very large specific surface, is better than the prepared nanometer sheet structure of prior art.The more important thing is zinc-aluminium duplex metal hydroxide nanometer sheet formed special three bit architectures that are interweaved, this has thoroughly solved the serious problem of reuniting and causing the specific surface of material significantly to reduce of the nano unit structure of ubiquitous zinc-aluminium double-metal hydroxide in prior art.Because the prepared 3D zinc-aluminium of the present invention double-metal hydroxide has larger specific area, the electric double layer capacitance amount of super capacitor part obviously increases.
(2), for electrode material, the mass transfer problem between electroactive composition and electrolyte is the key factor of determining electrode material property quality.The electroactive composition that only touches electrolyte is just brought into play useful effect, which is buried can not touch electrolyte electroactive composition in material internal to the charge-discharge capacity of super capacitor without any contribution.Involved in the present invention to 3D zinc-aluminium double-metal hydroxide there is unique space structure, it carries out electrochemical reaction flourishing mass transfer channel network is provided for power on active component and electrolyte of electrode on interface, make electrolyte can be deep into material internal and fully contact with the basic structural unit-nanometer sheet of electrode material, its mass transfer rate is apparently higher than prior art.Thereby cause the electric double layer capacitance amount part of super capacitor obviously to increase.
(3) for super capacitor material, existing double-metal hydroxide technology of preparing synthesis cycle is long, and synthesis step is loaded down with trivial details, and productive rate is undesirable, thereby has limited its industrialized production and application.The present invention utilizes microwave technology, has significantly reduced the synthesis cycle of material, and less energy consumption, and cost is low, and step is simple, environmental protection.The more important thing is that productive rate reaches 98%, improved significantly reaction efficiency, there is higher industrial applications prospect.
Embodiment
With embodiment, further illustrate the present invention below, but the present invention is not limited.The experimental technique of unreceipted actual conditions in the following example, conventionally according to normal condition, or the condition of advising according to manufacturer." room temperature " described in the present invention, " normal pressure " refer to temperature and the air pressure between regular job, are generally 25 ℃, standard atmospheric pressure.
In following embodiment, the electro-chemical test of electric capacity work electrode used is the foam zinc metal sheet (10mm * 10mm * 1mm) that scribbles composite material, to electrode, is platinum plate electrode (10mm * 10mm * 1mm), and reference electrode is saturated calomel electrode electrode.Electro-chemical test adopts time-measuring electric potential, and operating voltage is 0.0～0.4V, and constant current charge-discharge current density is 1.0A/g.
Embodiment 1
Take 0.582gZn (NO
3)
26H
2o and 0.873g Al (NO
3)
39H
2o is in 150mL absolute ethyl alcohol, open microwave reaction device, set 50 ℃ of reaction temperature lower limits, 80 ℃ of the upper limits, microwave power 200W left and right, stirring and dissolving reaction system is until system starts backflow, slowly dropwise add the pre-configured ethanol-ammoniacal liquor of 10mL (V: V=10: 1) mixed solution, regulate microwave power 250W left and right, control 0.5h and drip end, successive reaction 1h.Close and finish reaction, room temperature is cooling, vacuum filtration, and ethanol washing 5 times, 70 ℃ of dry 12h of vacuum, obtain 3D zinc-aluminium double-metal hydroxide.By 30mg3D zinc-aluminium double-metal hydroxide hollow microsphere and 5.6mg acetylene black ground and mixed, add a little polytetrafluoroethylene binding agent (15%), add a small amount of absolute ethyl alcohol, ultrasonic dispersion 30min, then above-mentioned material is coated in to foam zinc surface, at 60 ℃, vacuumize 12h, obtains electrode slice; Using resulting 3D zinc-aluminium double-metal hydroxide hollow microsphere electrode as work electrode with to electrode, and 6.0mol/L potassium hydroxide solution is electrolyte assembling super capacitor.Electrochemical property test shows, its specific capacitance is 401F/g, discharges and recharges after 1000 times, and capacitance keeps 96.2%.
Embodiment 2
Take 0.582gZn (NO
3)
26H
2o and 0.873g Al (NO
3)
39H
2o is in 150mL absolute ethyl alcohol, open microwave reaction device, set 60 ℃ of reaction temperature lower limits, 80 ℃ of the upper limits, microwave power 250W left and right, stirring and dissolving reaction system is until system starts backflow, slowly dropwise add the pre-configured ethanol-ammoniacal liquor of 10mL (V: V=10: 1) mixed solution, regulate microwave power 300W left and right, control 0.5h and drip end, successive reaction 1h.Finish reaction, room temperature is cooling, vacuum filtration, and ethanol washing 6 times, 70 ℃ of dry 12h of vacuum, obtain 3D zinc-aluminium double-metal hydroxide.By 30mg3D zinc-aluminium double-metal hydroxide hollow microsphere and 5.6mg acetylene black ground and mixed, add a little polytetrafluoroethylene binding agent (15%), add a small amount of absolute ethyl alcohol, ultrasonic dispersion 30min, then above-mentioned material is coated in to foam zinc surface, at 60 ℃, vacuumize 12h, obtains electrode slice; Using resulting 3D zinc-aluminium double-metal hydroxide hollow microsphere electrode as work electrode with to electrode, and 5.0mol/L potassium hydroxide solution is electrolyte assembling super capacitor.Electrochemical property test shows, its specific capacitance is 490.8F/g, discharges and recharges after 1000 times, and capacitance keeps 95.2%.
Embodiment 3
Take 0.582gZn (NO
3)
26H
2o and 0.873g Al (NO
3)
39H
2o is in 150mL absolute ethyl alcohol, open microwave reaction device, set 65 ℃ of reaction temperature lower limits, 80 ℃ of the upper limits, microwave power 300W left and right, stirring and dissolving reaction system is until system starts backflow, slowly dropwise add the pre-configured ethanol-ammoniacal liquor of 10mL (V: V=10: 1) mixed solution, regulate microwave power 350W left and right, control 0.5h and drip end, successive reaction 1h.Finish reaction, room temperature is cooling, vacuum filtration, and ethanol washing 8 times, 70 ℃ of dry 12h of vacuum, obtain 3D zinc-aluminium double-metal hydroxide.By 30mg3D zinc-aluminium double-metal hydroxide hollow microsphere and 5.6mg acetylene black ground and mixed, add a little polytetrafluoroethylene binding agent (15%), add a small amount of absolute ethyl alcohol, ultrasonic dispersion 30min, then above-mentioned material is coated in to foam zinc surface, at 60 ℃, vacuumize 12h, obtains electrode slice; Using resulting 3D zinc-aluminium double-metal hydroxide hollow microsphere electrode as work electrode with to electrode, and 4.5mol/L potassium hydroxide solution is electrolyte assembling super capacitor.Electrochemical property test shows, its specific capacitance is 485.8F/g, discharges and recharges after 1000 times, and capacitance keeps 96.2%.
Embodiment 4
Take 0.582gZn (NO
3)
26H
2o and 0.873g Al (NO
3)
39H
2o is in 150mL absolute ethyl alcohol, open microwave reaction device, set 70 ℃ of reaction temperature lower limits, 80 ℃ of the upper limits, microwave power 350W left and right, stirring and dissolving reaction system is until system starts backflow, slowly dropwise add the pre-configured ethanol-ammoniacal liquor of 10mL (V: V=10: 1) mixed solution, regulate microwave power 400W left and right, control 0.5h and drip end, successive reaction 1h.Finish reaction, room temperature is cooling, vacuum filtration, and ethanol washing 7 times, 70 ℃ of dry 12h of vacuum, obtain 3D zinc-aluminium double-metal hydroxide.By 30mg3D zinc-aluminium double-metal hydroxide hollow microsphere and 5.6mg acetylene black ground and mixed, add a little polytetrafluoroethylene binding agent (15%), add a small amount of absolute ethyl alcohol, ultrasonic dispersion 30min, then above-mentioned material is coated in to foam zinc surface, at 60 ℃, vacuumize 12h, obtains electrode slice; Using resulting 3D zinc-aluminium double-metal hydroxide hollow microsphere electrode as work electrode with to electrode, and 3.0mol/L potassium hydroxide solution is electrolyte assembling super capacitor.Electrochemical property test shows, its specific capacitance is 405F/g, discharges and recharges after 1000 times, and capacitance keeps 96.2%.
Embodiment 5
Take 0.582gZn (NO
3)
26H
2o and 0.873g Al (NO
3)
39H
2o is in 150mL absolute ethyl alcohol, open microwave reaction device, set 50 ℃ of reaction temperature lower limits, 80 ℃ of the upper limits, microwave power 400W left and right, stirring and dissolving reaction system is until system starts backflow, slowly dropwise add the pre-configured ethanol-ammoniacal liquor of 10mL (V: V=10: 1) mixed solution, regulate microwave power 500W left and right, control 0.5h and drip end, successive reaction 1h.Finish reaction, room temperature is cooling, vacuum filtration, and ethanol washing 10 times, 70 ℃ of dry 12h of vacuum, obtain 3D zinc-aluminium double-metal hydroxide.By 30mg3D zinc-aluminium double-metal hydroxide hollow microsphere and 5.6mg acetylene black ground and mixed, add a little polytetrafluoroethylene binding agent (15%), add a small amount of absolute ethyl alcohol, ultrasonic dispersion 30min, then above-mentioned material is coated in to foam zinc surface, at 60 ℃, vacuumize 12h, obtains electrode slice; Using resulting 3D zinc-aluminium double-metal hydroxide hollow microsphere electrode as work electrode with to electrode, and 6.0mol/L potassium hydroxide solution is electrolyte assembling super capacitor.Electrochemical property test shows, its specific capacitance is 500.2F/g, discharges and recharges after 1000 times, and capacitance keeps 96.2%.
Claims (8)
1. the invention provides a kind of microwave preparation of 3D zinc-aluminium double-metal hydroxide and the application in ultracapacitor, comprise
1) by zinc and aluminium salt precursor body and organic solvent mixing, ultrasonic dispersion, is transferred in microwave reaction device.Set reaction temperature, microwave power and reaction time, open microwave, stir until system starts to reflux.
2) alkali source compound and organic solvent are mixed, are added to 1) in the backflow system of reacting, after stirring reaction, centrifugation, collecting precipitation, absolute ethanol washing, vacuumize.
3) by 2) the 3D zinc-aluminium double-metal hydroxide that makes, acetylene black and polytetrafluoroethylene mix, and stirs, and be then applied to foam zinc surface, and be assembled into ultracapacitor.
2. the method for claim 1, is characterized in that, described microwave reaction device refers to can launch stability microwave and with all kinds of devices of agitating function.
3. the method for claim 1, is characterized in that, described organic solvent is any of absolute ethyl alcohol, propyl alcohol, isopropyl alcohol or the tert-butyl alcohol, or their mixture.
4. the method for claim 1, is characterized in that, described alkali source compound is to be selected from any in the organic or inorganic compound that can decompose rapidly and discharge ammonia under hydrothermal condition, or their mixture.
5. the method for claim 1, is characterized in that, described zinc and aluminium salt precursor body are to be selected to contain any in positive divalent zinc ion or the positive aluminum ions sulfate of divalence or nitrate.
6. the method for claim 1, is characterized in that, the amount of substance ratio of described zinc and aluminium salt is 3: 1～1: 3.The mass ratio of described zinc and aluminium salt precursor body and organic solvent is 1: 50～1: 150.Described alkali source compound and the volume ratio of organic solvent are 1: 10～1: 20.Described microwave reaction temperature and time is respectively 50～80 ℃ and 0.5～1.0h.
7. the method for claim 1, is characterized in that, the mass ratio of described 3D zinc-aluminium double-metal hydroxide and acetylene black, polytetrafluoroethylene is 1: 0.3: 0.15～1: 0.1: 0.05.
8. the method for claim 1, is characterized in that, the barrier film that described assembling super capacitor is used is to be selected from any in the barrier film series that polypropylene material makes.The potassium hydroxide solution that the electrolyte that described assembling super capacitor is used is 3～6mol/L.
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102496480A (en) * | 2011-12-16 | 2012-06-13 | 江南大学 | Preparation method of graphene/nickel-aluminum bi-metal hydroxide composite material and application thereof |
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2013
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102496480A (en) * | 2011-12-16 | 2012-06-13 | 江南大学 | Preparation method of graphene/nickel-aluminum bi-metal hydroxide composite material and application thereof |
Non-Patent Citations (3)
| Title |
|---|
| JIHONG FANG等: "Microwave-assisted synthesis of CoAl-layered double hydroxide/graphene oxide composite and its application in supercapacitors", 《ELECTROCHIMICA ACTA》 * |
| 刘献明等: "CoAl 双氢氧化物作超级电容器的电极材料", 《电源技术》 * |
| 李龙凤等: "微波加热回流法合成Mg-Al 二元类水滑石化合物", 《淮北师范大学学报》 * |
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Application publication date: 20140910 |